Carboxylated organic-inorganic hybrid monolithic column as well as preparation method and application thereof
A carboxylation and monolithic column technology, applied in the field of detection, can solve the problems of poor stability of the carboxylated monolithic column, cumbersome preparation process, low reproducibility, etc., and achieves cheap and easy-to-obtain reagents, good repeatability, and low column pressure. Effect
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[0045] Such as figure 1 As shown, a method for preparing a carboxylated organic-inorganic hybrid monolithic column of the present invention comprises the following steps:
[0046] S10, activate the capillary, intercept the capillary of 5-10cm, use 1.5mol L successively -1 NaOH solution (12h), water (30min), 1.5mol L -1 Rinse with hydrochloric acid solution (12h), water (30min), methanol (30min), then blow dry with nitrogen, and set aside;
[0047] S20, mixing the raw material mercaptosuccinic acid providing carboxyl and mercapto functional groups with initiator, porogen, and acid-base regulator in a centrifuge tube to obtain a mixed solution of mercaptosuccinic acid, wherein the acid-base regulator is ammonia water and urea The mixture, the initiator is 2,2'-azobisisobutyronitrile hydrochloride; the porogen is polyethylene glycol-20000, polyethylene glycol-8000, hexadecyl trimethyl bromide One or more of ammonium, preferably the porogen is polyethylene glycol-20000;
[004...
Embodiment 1
[0060] Taking three actual environmental water samples as examples, the water from the Yangtze River, Jiuxiang River and Yangshan Lake were all collected from Nanjing, Jiangsu Province. After passing through a 0.45 μm filter membrane, the concentration of inorganic chromium was determined.
[0061] The application of a carboxylated organic-inorganic hybrid monolithic column in this embodiment in the separation and enrichment of inorganic chromium, the specific steps are:
[0062] 1. Preparation of carboxylated organic-inorganic hybrid monolithic column
[0063] The specific steps are:
[0064] S10, 42.6mg of mercaptosuccinic acid (MSA), 1.5mg of 2,2'-azobisisobutyronitrile hydrochloride (V 50 ), 0.225mL ammonia water (NH 3 ·H 2 O), 0.4mL H 2 0.60mg polyethylene glycol-20000 (PEG-20000), 75mg urea are mixed in the 1.5mL centrifuge tube, obtain the mixed solution of mercaptosuccinic acid;
[0065] S20. Add 0.2 mL of tetramethoxysilane (TMOS) and 0.1 mL of γ-methyl methacryl...
Embodiment 2
[0078] The basic content of this example is the same as that of Example 1, except that in this example, the molar ratio of MSA to γ-MAPS is 1:1, the molar ratio of TMOS to γ-MAPS is 1:2.7, ammonia water and γ-MAPS The mass ratio of MAPS is 2:1, the mass ratio of urea to MSA is 1.5:1, V 50 The dosage of PEG-20000 is 1% of the total mass of MSA and γ-MAPS, and the dosage of PEG-20000 is 1.5 times of the mass of MSA. The obtained carboxylated organic-inorganic hybrid monolithic column has good permeability and stability.
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